Associated and natural gas conversion process

FIELD: oil and gas industry.

SUBSTANCE: invention is referred to conversion process of associated and natural gases with high content of heavy methane homologs by direct partial oxidation of hydrocarbon gas and further carbonylation of the received products. At that hydrocarbons gas is mixed up with oxygen or oxygen-containing gas with mole ratio of hydrocarbon in heavy components: oxygen of 10-1:1 and selective oxidation of heavy components is made at temperature of 350-420°C and pressure of 10-40 bar and the received products are subjected to processing in presence of carbonylation catalysts with production of liquid products of carboxylic acids and their ethers and dry fuel gas purified from heavy components and enriched with methane.

EFFECT: method is the simplest and the most economically feasible for processing of associated oil gas and natural gas with high content of methane homologs with production of dry gas and a range of valuable liquid products.

3 ex

 

The invention relates to the oil and gas industry, in particular to the processing of petroleum and natural gases with a high content of homologues of methane in chemical products. These gases are valuable hydrocarbons, but in many cases do not find practical application and is often flared. Associated gas is difficult to transport and difficult to use without further processing or purification from the contained heavy components3+homologues of methane. The problem of utilization of associated petroleum gas is standing in front of all oil companies. For oil transportation and processing of associated petroleum gas for further use unprofitable, as the cost of such fuel, as a rule, exceeds the market.

Known methods of processing of petroleum and natural "fatty" gases using physical separation methods - absorption, compression and separation, distillation and other So-known method of extraction of hydrocarbons From3+of associated petroleum gas by countercurrent absorption absorption with subsequent desorption of the absorbed fraction With3+and returning the regenerated after desorption of the absorbent in the absorber, characterized by the fact that the use of associated petroleum gases by compression 8-20 ATM, and the absorption is carried out at a temperature of 8-40°C, while leaving the absorber rich absorbent is heated to 280-350°C and is fed to the desorption being carried out at a pressure of 15 to 19 atmospheres, and in use as an absorbent of heavy components of the source gas (RF Patent 2338734 (2007)). The disadvantages of this method are the complexity of the process, the high cost of equipment and the need for additional energy consumption for regeneration of the absorbent.

A method of refining petroleum gas, comprising compressing the original petroleum gas, its cooling and separation from getting dry gas and gas condensate, in which a two-stage separation, gas condensate is subjected to distillation in a distillation column to obtain propane-butane fraction and stable gas condensate and propane-butane fraction is cooled and condense (RF Patent 2340841 (2007). The disadvantage of this method is the large additional energy consumption for gas compression.

There are also known methods of processing of petroleum and natural "fatty" gases, comprising the additional step of chemical processing "heavy" components of hydrocarbon gases. So, in the process using a hydrocarbon feedstock containing higher hydrocarbons, comp is the s Haldor-Topsoe are pre-reforming of hydrocarbons at temperatures of about 450-550°C. In the process of prereforming with steam due to steam reforming With3+the hydrocarbons in these conditions is the clean methane gas from these connections and provides subsequent steam methane reforming without pitch and coking of catalysts for production of synthesis gas (RF Patent 2263627 C2 (Haldor, Topsee) (2000). The disadvantages of this method are significant cost and complexity to the equipment due to the introduction of an additional stage of prereforming and additional energy consumption at this stage.

There is also known a method for co-processing of liquefied petroleum gas (LPG) and field preparation of the products of oil or gas condensate fields with the receipt of the products transported together with trademarks oil and commodity gas, namely the processing of liquefied petroleum gas (LPG) in a mixture of aromatic hydrocarbons (aromatic concentrate). The method includes commercial preparation of associated petroleum gas (APG) or "sour gas" with obtaining commercial dry gas and gas condensate, supply of condensate on the stage of stabilization with the release of the gas condensate liquefied petroleum gas (LPG), the reaction conversion of LPG in a mixture of aromatic hydrocarbons in a hundred is AI platforming, separation of the reaction products platforming on hydrogen, hydrocarbon gas and liquid products of the reaction, the liquid reaction products produce aromatic hydrocarbons, which are served in the main oil pipeline in the composition of the crude product (RF Patent 2435827 (2010)). The disadvantages of this method are complex technological scheme of the process, the cost and complexity of the equipment due to the stage of prereforming and high energy consumption for the process.

There is a method of preparation of associated crude oil and natural gas for use in reciprocating internal combustion engines (EN 2385897, C10L 3/10, F02M 31/00, 10.04.2010), which is that produced gas in a mixture with oxygen-containing gas such as air, is subjected to heat treatment at a temperature of 450-1100°C for 0.01 to 50 when the content of free oxygen in the mixture is 0.5-5%. Heat treatment may also be carried out in the presence of catalysts of the oxidative condensation of methane, steam, carbon dioxide reforming of methane oxidative dehydrogenation of lower alkanes or combinations thereof. As reaction promoters may act nitrogen oxides, hydrogen peroxide, halogen compounds, unsaturated or oxygen-containing hydrocarbons or reduce the likelihood of sooting (water vapor). As a result, when specified the conditions there is practically no conversion of lighter hydrocarbons 1-C4, while the conversion of hydrocarbons With5+that has a very low methane number, greater than 95%. The main products of transformation With5+hydrocarbons such heat treatment of associated petroleum gases are (in descending order of output) ethylene, methane, ethane and carbon monoxide. This provides selective conversion of compounds having a low knock resistance and increases the probability of tar and soot formation, and there is an increase in methane number get gas. Despite the fact that the above method cannot convert the hydrocarbons5+the drawback of this method is the low conversion2-C4components of associated petroleum gas with a low methane number compared to pure methane. For example, propane and butane are methane, 35 and 11, respectively, and, even in small quantities mixed with methane, greatly reduce its methane number. For example, a mixture of 95% methane, 3% propane and 2% butane methane number is equal to 72. In addition, for their own energy consumption and crafts can be used only a small part of the produced associated gas (less than 20%).

Known processing "dry" (methane, without impurities With2+hydrocarbons) of natural gas, including obtaining methanolate dimethyl ether from synthesis gas and subsequent processing of methanol or dimethyl ether by carbonyliron in acetic acid and/or methyl acetate in the liquid or vapour phases.

For the implementation of the carbonyl process proposed catalysts based on acidic cesium salts fosfornomolibdenovoi heteroalicyclic promoted with rhodium, the activity of which is 190 g/l cat.h) [RF Patent 2170724, G. G. Volkova, L. M. Plyasova, A. N. Salanov, G. N. Kustova, T. M. Yurieva and V. A. Likholobov, C07C 67/36, B01J 31/16, 20.07.2001)], the lack of which was the use of an expensive component in the catalyst is rhodium, which leads to a significant increase in the cost of the catalyst and the appreciation of the whole process.

Known catalyst and method for producing methyl acetate (RF Patent 2422203) without the use of rhodium and iodide promoters by carbonylation of dimethyl ether at a temperature of 200-250°C, a pressure of 10-20 ATM, in the presence of a catalyst comprising an acidic cesium salt fosfornomolibdenovoi heteroalicyclic composition: CsxHyPW12O40where: 1.3≤x≤2.2, y=3, with the addition of platinum in an amount of from 0.25 to 1.0 wt.%. However, this method is not aimed directly at solving the task of creating a simple and economical method of processing petroleum and natural "fatty" gases, and describes one of the possible stages of their processing.

The closest, albeit indirect analogue containing some signs, matching us with the claimed invention, is patent US 5659077 from 19.08.97 in which the proposed company is exny the process of conversion of methane into acetic acid and/or methyl acetate by partial oxidation of methane, bypassing the stage of synthesis gas. Direct oxidation of methane with a methane conversion in a single pass through the reactor 6-12% is carried out at temperatures above 425°C and a working pressure of ~70-100 bar. Dedicated methanol and the extension number of purchased methanol at the same pressure and T=180-250°C Carboniferous carbon monoxide formed in the reaction gases of the oxidation process, in acetic acid to rhodium catalyst in the presence of CH3I. the Shortcomings of the proposed method are: the need to implement the process of partial oxidation at high pressure (~70-100 bar), recycling of a significant amount of unreacted methane, a large accumulation of carbon dioxide and the necessity of removing the excess scrubbing cleaning recirculating flow, as well as the fact that it is designed to use only "dry" methane gas that is not offered by us provides technical result aimed at processing the hydrocarbon gas complex composition with obtaining enriched in methane and purified from heavy gas components for power plants and simultaneous achievement of esters of carboxylic acids.

The objective of the invention is to provide a simple and economical method of processing petroleum and natural gases with a high content of homologues of meth is on obtaining purified dry gas and a number of valuable liquid products.

The problem is solved by the claimed method of processing petroleum and natural gases with a high content of heavy homologues of methane by direct partial oxidation of the hydrocarbon gas and the subsequent carbonylation products, in which hydrocarbon gas is mixed with oxygen or oxygen-containing gas in a molar ratio of carbon heavy components:oxygen 10÷1:1 and carry out the selective oxidation of heavy components at a temperature of 350-420°C and a pressure of 10-40 bar, and the resulting products are treated in the presence of catalysts for the carbonylation of obtaining liquid products from a number of carboxylic acids and their esters and enriched in methane cleared of heavy components of the dry fuel gas. Unreacted methane and an additional amount of methane formed during the oxidation of heavy gas components, and further specified the reaction mixture is subjected to additional treatment in the presence of catalysts for the carbonylation of obtaining liquid products from a number of carboxylic acids and their esters and enriched in methane cleared of heavy components of the fuel gas for power generation. Carbonylation is conducted by known techniques in the vapor or liquid phase with a preliminary allocation of methanol with or without highlighting.

Thanks to the Yu partial oxidation at a temperature of 350-420°C and a pressure of 10-40 bar, that is, in a milder conditions compared with the equivalent, is provided by selective oxidation of only hydrocarbons With3+while methane under these conditions is not oxidized, and even, on the contrary, additionally produced along with the main products of partial oxidation of hydrocarbons With3+methanol, ethanol, WITH. These products together with unreacted methane is further treated with participation of well-known catalysts for carbonylation, however, interacts with alcohols to obtain carboxylic acids and their esters, which condense with obtaining an aqueous solution of these compounds, and in the form of a gas-phase product get refined heavy component hydrocarbon gas with a higher methane number compared to the baseline petroleum gas, which can be used as fuel for power plants. An aqueous solution of carboxylic acids and their esters can be further fractionated by known methods of obtaining individual target components, or used directly in the oil industry.

Examples of the implementation of the proposed method.

Example 1. The mixture of hydrocarbon gases composition: SN4- 90.7 percent, With2H6of 1.8%, With3H8- 5,3%, With4H10is 2.2% (methane number 64) at a pressure of 40 bar in the amount of 0.35 nm3/h on remaut to a temperature of 350°C and subjected to three-step oxidation by oxygen, served in a number of 18.4 l/h for each stage of oxidation, a total of 55.2 l/h ratio (carbon heavy components:oxygen ~ 1:1). In the partial oxidation receive the gas mixture in the amount of 0.39 nm3per hour, containing 41.8 g of methanol and 28.3 g of carbon monoxide. The mixture is cooled to a temperature of 180-250°C and subjected to carbonyliron in a known manner, where 98% conversion of methanol and selectivity 99% receive of 62.4 g/h of a mixture of acetic acid and methyl ester of acetic acid, and 0.34 nm3enriched with methane gas with a methane number 78.

Example 2. The mixture of hydrocarbon gases composition: SN4- 81%, With2H6is 3.2%, With3H8compared to 12.1%, With4H10to 3.7% (methane number 52) at a pressure of 20 bar in the amount of 0.32 nm3/h was heated to a temperature of 370°C and subjected to two-stage oxidation with oxygen, which serves in the amount of 16.8 l/h for each stage of oxidation, a total of 33.6 l/h ratio (carbon heavy components:oxygen is ~ 5:1). In the partial oxidation receive the gas mixture in an amount of 0.34 nm3per hour, containing 24 g of methanol and 14.7 g of carbon monoxide. The mixture is cooled to a temperature of 180-250°C and subjected to carbonyliron in a known manner, where 98% conversion of methanol and selectivity 99% get 35,8 g/h of a mixture of acetic acid and metrolog the ester of acetic acid, and 0.31 nm3enriched with methane gas with a methane number 56.

Example 3. The mixture of hydrocarbon gases composition: SN4- 81.7 per cent, With2H6at 3.7%, With3H8to 11.2%, With4H10and 3.4% (methane number 53) at a pressure of 10 bar in the amount of 0.3 nm3/h heated to a temperature of 420°C and subjected to oxidation with oxygen, which serves in the amount of 15.8 l/h ratio (carbon heavy components:oxygen is ~ 10:1). In the partial oxidation receive the gas mixture in the amount 0,31 nm3per hour, containing 11.3 g of methanol and 6.9 g of carbon monoxide. The mixture is cooled to a temperature of 180-250°C and subjected to carbonyliron in a known manner, where 98% conversion of methanol and selectivity of about 99% get to 16.8 g/h of a mixture of acetic acid and methyl ester of acetic acid, and 0.3 nm3enriched with methane gas with a methane number 55.

The method of processing natural gas and associated petroleum gas with a high content of heavy homologues of methane by direct partial oxidation of the hydrocarbon gas and the subsequent carbonylation products, characterized in that the hydrocarbon gas is mixed with oxygen or oxygen-containing gas in a molar ratio of carbon heavy components:oxygen 10÷1:1 and carry out the selective oxidation of heavy components at a temperature of 350-420°C and a pressure of 10-40 bar, and the resulting products are treated in the presence of catalysts for the carbonylation of obtaining liquid products from a number of carboxylic acids and their esters and enriched in methane cleared of heavy components of the dry fuel gas.



 

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FIELD: chemistry.

SUBSTANCE: invention relates to methods of obtaining esters of amyl alcohols and simplest carboxylic acids C1-C4. Alcohol-containing wastes of caprolactam production are used as raw material. Method includes etherification of alcohol-containing wastes of caprolactam wastes with simplest carboxylic acids C1-C4 in presence of acidic catalyst. Process of etherification is carried out with continuous azeotropic distillation of water with reaction mixture components, as catalyst, sulfuric or orthophosphoric acid is used, catalyst is loaded in amount 0.1-2.5% of the total weight of initial substances, reaction mixture is cooled to 20-30°C and neutralised with water-alkaline solution with mixing to water layer pH 7-8, water phase is separated, organic phase is washed one-two times with water, final purification of esters is carried out by fractional distillation of organic phase. Obtained products are suitable for application as solvents for paints and varnishes, raw material for organic synthesis, as component of complex fuel additives.

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FIELD: chemistry.

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17 cl, 5 dwg, 1 tbl, 4 ex

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10 cl, 4 ex, 1 dwg, 1 tbl

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14 cl, 9 ex, 4 dwg, 1 tbl

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17 cl, 5 dwg, 1 tbl, 4 ex

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2 cl, 5 ex

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41 cl, 2 tbl, 18 ex

FIELD: chemistry.

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28 cl, 3 tbl, 3 ex

FIELD: chemistry.

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28 cl, 1 tbl

FIELD: chemistry.

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5 cl, 9 ex, 1 tbl

FIELD: chemistry.

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6 cl, 2 ex

FIELD: chemistry.

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22 cl, 3 tbl, 5 ex

FIELD: chemistry.

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EFFECT: method is characterised by improvement of catalytic activity.

15 cl, 3 tbl, 3 ex

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